Recovery of basic calcium hypochlorite compounds



Patented June 3, 1941 mien? RECOVERY OF BASIC CALCIUM HYPO- CHLORI'DE COMPOUND-S Heinrich Reitz and Hans Ehlers, Bitterfeld, Germany, assignors, by mesne assignments, to Pen- Chlor, Incorporated, Philadelphia, Pin, a corporation of Delaware No Drawing. Application May 24, .1938, Serial No.

209mm. In Germany June 8, 1937 '2 Claims.

This invention relates to a process for the production of basic calcium hypochlorite compounds.

In accordance with a known process, basic calcium hypochlorites can be precipitated from lyes which contain calcium chloride in addition to available chlorine, by the addition of lime. Such lyes are produced, for example, when chloride of lime (bleaching powder) is treated with water to produce a slurry; they are also obtained in the form of a mother liquor in the production of calcium hypochlorite by the chlorination of concentrated lime slurries until neutral calcium hypochlorite is precipitated, after separation of the greater extent than when working at ordinary temperature, since 80% and more of the available chlorine of the originating lye is recovered in the form of basic calcium hypochlorite compounds. These differences in behaviour are apparently due to the fact that the hot lye containing calcium chloride and calcium hypochlorite possesses a greater solvent power for calcium hydrate.

In spite of the higher range of temperatures employed in the present process, no noticeable loss of available chlorine occurs through the decomposition of hypochlorite.

The addition of lime is preferably so proporlatter. These lyes constitute solutions of calcium tiOfled that 2 mOlS- of Calcium hydrate a e a d d chlorid whi h are saturated th calcium hypofor 1 mol. of available chlorine contained in the chlorite. The problem of recovering the availlye to be treated. The calcium hydrate may be able chlorine still contained in lyes of this kind, added in t form of a dry powder; it s w v r is of considerable importance to the economy of p e e le to add i s an q e s p n n in processes of the foregoing ki d, the proportion of about 6 parts by weight of The recovery of the available chlorine content Water o 5 parts by weight of calcium hydrate, of such lyes by precipitation with lime has, in whereby the filtrability of the product is further practice, however, always failed hitherto owing improvedto the fact that the precipitated basic calcium T e following examp Will Serve t0 illustrate hypochlorite compounds which initially form a the p s of e present invention! fine-powdery deposit, rapidly cake together into Exam ple I more or less cohesive masses, so that their separation from the mother lye becomes impracti- 1000 parts by volume, corresponding to 1307 cable; while in consequence of their greatly varyparts y w i f a y containing l i m h p ing content of free calcium hydrate, they possess chlorite and calcium chloride, comprising 272 an indefinite composition. grms. per litre of total chlorine and 96 grms. per

It is an object of the present invention to imlitre of available chlorine, were suspended in the prove the aforesaid known process in such a mansame amount by Weight o Water, W h the add ner that the basic calcium hypochlorite precipition of 100 parts by weight of calcium hydrate, tates retain their original fine-powdery or granuheated to 80-90 C. and centrifuged While still lar condition so as to enable them to be easily hot. 530 parts by weight of filter cake, containseparated from the calcium chloride mother lye. ing 6% parts y Weight) f va b It has now been ascertained in accordance with chlorine and 730 parts by volume of mother lye the present invention that the solidification of containing 6 grms. per p s y the deposit is due to the presence therein of cal- Weight of available chlorine were obtained. Of cium oxychloride, which is formed at the tem- 40 the 96 grms. per litre of available chlorine conperatures employed, and that the foregoing drawbacks may be avoided by treating solutions of the first mentioned type with lime at temperatures above about 40 C., preferably at from 80 to tained in the originating lye, 84.6 grms.. per litre-:89% were thus recovered in the solid product obtained. Analysis of the latter gave the following figures:

90 C. The hardening of the precipitated com- Per cent pounds is thus avoided, and, on the contrary, Available chlorine content 34.4 readily filtrable basic calcium hypochlorite com- Total chlorine content 23.5 pounds are formed, which remain powdery or 090 30.5

fine-grained, and the lime content of which is in complete accordance with the theoretical content following from the known solubility of the basic hypochlorite compounds, and of hydrate of lime, respectively. Moreover, when working in this manner, the available chlorine content of the residual lye is reduced to a considerably Example II 1000 parts by volume of a lye containing 286 grms. per litre of total chlorine and 100.8 grins. per litre of available chlorine were mixed with 121 parts by weight of calcium hydrate and heated to C. After separation of the precipitate tion to available chlorine, which comprises causing calcium hydrate to react with such lyes at temperatures from about 80 to about 90 0., and thereafter separating the precipitated basic calcium hypochlorite compounds from the residual lye while maintaining such temperatures.

2. A process for the recovery of calcium hypochlorite compounds from solutions containing substantial amounts of calcium chloride in addition to available chlorine, which comprises adding an aqueous suspension of calcium hydrate to such lyes so as to cause reaction between the available chlorine content of the lye and the calcium hydrate at temperatures from about 80 to about 90 C., and thereafter separating the precipitated basic calcium hypochlorite compounds from the residual lye while maintaining such temperatures.

HEINRICH REITZ.

HANS EHLERS. 

